Process for the manufacture of lighter colored products from earth oil residues, asphalt, and/or similar substances



Patented July 19, 1 932.

UNITED STATES, PATENT orrlca uconus wrtnnmms m NOBEL, or AMSTERDAM, NETHERLANDS, assrenon '10 ml BATAAISGHE rnrnonnun maarscnarrra, or ran HAGUE, un'rnnnmuvns HOGESS FOR THE MANUFACTURE OF LIGHTER COLORED PRODUCTS FROM EARTH OIII RESIDUES, ASPHALT, AND/OR SIMILAR SUBSTANCES 1T0 Drawing. .Applicationfiled November 2, 1928, Serial No. 316,8 85, and in the Netherlands June 11, 1988.

The invention relates to a process for the manufacture of lighter colored products from petroleum residues, 'asphalts and/or similar substances.

6 It is known that nearly all the asphalts whether occurrin in natural state or obtained in an arti cial way possess a black or substantially black color. Even when light passes through very thin layers of 10 the asphalt it still has a very dark tone.

For certain purposes, however, a lighter colored asphalt is desired. For instance, 1t is desirable to have asphalts having a lighter tone for the production of light colored emulsions or gels, or for the manufacture of asphalt paper, lacquers, varnishes, asphalt paints, etc.

Up till now, -for the said purposes, only a 1i ht colored asphalt was available, which I is 0 tained as a residue, when certain crude petroleums, which are found only sporadically, are distilled.

According to the present invention means are provided which render it possible to prepare from any asphalt, even the darkest and heaviest ones, and both from artificial ashalt, i. e. residues obtained by the distilation of crude petroleum as well as from natural asphalt, a product which has a light- 8 er color than the original asphalt, without impairing the properties which asphalt should have for industrial purposes. Itis also possible to prepare the said lighter colored products by starting from petroleum residues and the like. The products prepared according to the present invention are equivalent to the known light colored asphalt above mentioned and it is even easily possible to obtain a product that is, still lighttake place that, in the first place, the greater part of the substances present in the asphalt would be removed and in consequence thereer in color and meets the highest requireof the ield of the process be decreased so much t at 1t would be uneconomical, and

in the second place, the refined product would be changed to such an extent, that it would have lost its asphalt character totally.

It has been found, however, that it is quite possible to prepare a lighter colored product from dark asphalt without thereby causlng such changes in the mass that the final product is useless, technically, and morev I phaltenes in the description and claims. It

is pointed out, however, that although the substances which are removed according to the invention for the greater part belong to the group of compounds which are named asphaltenes in asphalt chemistry and are considered as being characteristic constitucuts of asphalts, the word asphaltenes as willbe used further in the description and claims has a somewhat larger meaning. For instance it may happen that in order to prepare a light colored product from asphalt, it is-necessary to remove from it not only the true asphaltenes but also other substances which do not possessthe characteristic properties of the asphaltenes. As these constituents of asphalt, however, are not scientifically determined (the asphaltene content of one and the same asphalt is stated very difierently by various investigators) we must suflice with the expression asphaltenes.

According to the invention the asphaltenes may be removed by treating the petroleum resldue, the asphalt and similar substances with a reagent which will precipitate the asphaltenes whether or not in the presence of a diluent.

Asreagents which will precipitate the asphaltenes various substances may be used,

as for example gasoline poor in aromatic constituents, pentane and other light hydrocarbons poor in aromatic constituents, while benzine, kerosene, etc., may serve as dlluents. Of course it is also possible that a liquid may serve simultaneously as a diluent and as a precipitating reagent.

Furthermore it was found, that the asphaltenes may be removed by treating the starting material with certain chemical substances, e. g. sulphuric acid, anhydrous ferric-chloride or anhydrous stannic-chloride, which convert the asphaltenes wholly or for the greater part into insoluble compounds. Also this treatment may, if desired, take place in the p esence of a diluent. It is not quite certain, whether, in adding the sulhuric acid or other substances which act 1n the same way, the total amount of the asphaltenes is converted into insoluble compounds or that only a part of them is indeed chemically affected and that the. finely divided asphaltenes which are not chemically afiected are occluded by the precipitate or the acid tar. In any event this treatment affords a mass which may be readily filtered and which furnishes, after separation of the insoluble constituents, a lighter colored filtrate.

According to the invention the asphaltenes may be further totally or partly removed by treating the starting material with a decolorizing powder whether or not in the presence of a diluent. Various well-known decolorizing powders may be used e. g. bleaching clay, decolorizing carbon, etc.

Very satisfactory results may be obtained according to the invention by subjecting the starting material to a combined treatment with a precipitating reagent and a chemical reagent which is able to convert the asphaltenes into insoluble compounds.

Sometimes it is advantageous to combine thetreatment with a precipitating reagent with a treatment which consists in removing the asphaltenes with the aid of a decolorizing powder. Furthermore it is also possible to combine the last mentioned treatment with a treatment with a chemical reagent, whereby no precipitating reagent is used.

If the starting material is subjected to a treatment according to which a precipitating reagent as well as a chemical reagent for converting the asphaltenes into insoluble compounds and a decolorizing powder is applied a very intensive decolorizing action may be produced. I

The order in which the succession of the elementary treatments described above will take place, depends on circumstances; it is also possible to perform two or more of the treatments simultaneously.

Furthermore it was found that if an asphalt, a petroleum residue or a similar substance has been converted into a lighter (:01-

ored product, the latter may be given the consistency of an asphalt or of an asphalt of lower penetration (higher melting point) without impairing the light color which is obtained by the treatment according to the invention by concentrating, e. g. by distillation with steam, either with or without the use of reduced pressure or vacuum.

Thus the invention allows the preparation from any given asphaltic residue, asphalt and the like, of light colored asphalts of the desired penetration.

In order that the invention may be more clearly understood .the following examples are given; it is however pointed out that the invention is notat all limited to the processes set forth inthe examples.

Ewample I 100% sulphuric acid by weight of the asphalt is then added to the mixture while stirring. The mass is allowed to settle and the acid tar and occluded substances are removed. While agitating now 3% bleaching clay (Terrana) is added, the mass being main: tained at a temperature of approximately C. Directly after the treatment with Terrana the mass which then ma have a temperature of say 40 C. is passe through a filter press, thereby removing the Terrana and sludge; finally the benzine is distilled off and the asphalt is brought on the desired penetration by means of a steam distillation. The color of the asphalt obtained resembles in all respects the well known light colored asphalts and it is equally suitable for the manufacture of emulsions, gels and other applications.

Example I I Ewample I I I A Californian asphalt is agitated with the same quantity of benzine while heating to approximately 60 C. until the asphalt is homogeneously dissolved. Then a fourfold quantity of pentane (with respect to the quantity of asphalt) is added and the mass allowed to cool. After settling of the asphaltenes the mass is filtered and the pentane and benzine are distilled ofi'. The resulting lot mass shows a considerably lighter color compared with the original asphalt.

. Example IV f A Sumatra asphalt is treated at about 80 C. with a twofold quantity motorkerosene, which acts as a diluent. The mass is then cooled to a temperature of approximately 60 C. andthereafter treated with 8 percent of 100% sulfuric acid by weight of the asphalt. When the mass is cooled the acid tar is settled. The acid tar may be removed by decantation, filtration and washing. After distilling off the kerosene with the aid of steam the final product is obtained having a brown color.

Ewample V A Borneo asphalt is dissolved in the twofold quantity of petrolspirit boiling from 100130 0., which acts as a diluent but which at the same time part-1y precipitates the asphaltenes. After treating the mass at 50 C. with 5 percent of 100% sulphuric acidby weight of the asphalt the acid tar is allowed to settle and is removed. By distilling off the petrol from the filtered solution with the aid of steam the lighter colored final product is obtained.

Example VI The solution obtained according to the foregoing example after removing the acid tar is treated at approximately C. with 5% Terrana bleaching clay by weight of the asphalt and then filtered. Thereafter the petrolspirit is distilled off with the aid of steam. The final product is somewhat lighter colored than the asphalt obtained according to Example V.

Emmple VII Borneo asphalt is dissolved at about C. in petrolspirit boiling from 60-80 C. The mass is then cooled to a temperature of say 40 C. and while agitatin 5% stannicchloride by weight of the asp alt is added. The deposited substances are filtered off from the warm liquid which thereafter is heated to distill off the petrolspirit. A very light colored asphalt is obtained.

Example VIII In the above examples the concentration of sulphuric acid may vary from to Of course for each starting material different quantities of substances to be applied will be required which may be determined experimentally in each case.

In the first place these quantities substantially depend on the as haltene content. But even the heaviest and arkest asphalt may be converted into a lighter colored product with the aid of only relatively small quantities of the said substances.

If a liquid with a higher boiling point is used as a diluting agent for instance kerosene, it is preferable to perform the distillation with the aid of steam, which has a favorable influence on' the color of the resulting product.

It should be well understood that if in the claims the expression in a liquid condition is used this may either mean that the asphalt, petroleum residues and the like are brou ht 1n a liquid condition by melting or by issolving the said substances in a suitable diluent. In the latter case it is not always necessary that the total quantity of the substances is dissolved, but generally the mass should be suificiently liquid'to allow the precipitation or conversion of the asphaltenes.

Having described my invention what I claim is: v

1. The process of producing lighter colored asphaltic products adaptable, for use in preparing light colored emulsions, gels, lacquers, varnishes, paints and the like, which consists in treatingdark colored asphaltic products, including petroleum residues with approximately 5% of stannic chloride, whereby on] 'the asphaltenes are removed from the dar colored asphaltic products.

2. The process of producing lighter colored asphaltic products adaptable for use .in preparing light colored emulsions, gels, lacquers, varnishes, paints and the like, which consists in treating dark colored asphaltic products, including petroleum residues, with a diluent and then with 5% of stannic chloride, whereby only the asphaltenes are removed from the dark colored asphaltic roducts.

3. The process of pro ucing lighter colored asphaltic products adapted foruse in preparing light colored emulsions, gels, lacquers, varnishes, paints and the like, which comprises treating dark colored asphalt with a substance containing a mineral acid radical, whereby the asphaltenes are precipitated while the resins present in the asphaltic products remain unaffected, and concentrating the mass.

4. The process as set forth in claim 3 in which the asphaltenes are precipitated by adding 2 to 8% of a 100% sulphuric acid solution.

5. The process of producing lighter colored asphaltic products adapted for use in preparin light colored emulsions, gels, lacquers, varnis es, paints and the like which comprises treatmg dark colored asphalt with sul-' phuric acid 1n the presence of a diluent whereby the asphaltenes are precipitate while the resins present in the asphaltie products remain unafiected, treating the mass with a bleaching earth, filtering, recovering the filtrate and concentrating the same.

6. The process of producing lighter colored asphaltic roducts adaptable for use in preparing lig t colored emulsions, gels, lacquers, varnishes, paints and the like, which comprises .heatmg a solid asphalt until it is in a molten condition, adding a li uid hydrocarbon, then adding approximate y 2% of sulphuric acid while stirring, then adding a bleaching earth, filtering the mass, removing the liquid hydrocarbon by distillation and concentrating the mass by steam distillation.

In testimony whereof I have aflixed my signature.

JACOBUS WILHELMUS m NOBEL. 

